KR910011744A - Direct esterification of more than 95% of the acid ends of diacids with glycol - Google Patents

Abstract

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Description

Direct esterification of more than 95% of the acid ends of diacids with glycol

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Claims (20)

(a) mixing the 1,4-butanediol and diacid in a molar ratio of 1,4-butanediol: diacid at least 2: 1 to form a reaction mixture, (b) heating the reaction mixture to about 180 ° C., ( c) adding 0.13 × 10 ⁻³ to 5.2 × 10 ⁻³ water of the catalyst compound selected from the group consisting of organo-tin, organo-titanium and organo-zirconium compounds per mole of diacid to the heated reactant, and ( d) reacting the reaction mixture under atmospheric pressure at an average reaction temperature of 180 ° C.-245 ° C. for a time not exceeding 60 minutes from the time the catalyst compound was added to the reaction mixture to form directly esterified diacid products. , For direct esterification of at least 95% of the acid ends of the diacids. (a) mixing the ethylene glycol and diacid in a molar ratio of at least 2: 1 ethylene glycol: diacid to form a reaction mixture, (b) heating the reaction mixture to about 180 ° C., (c) organic per mole of diacid Adding 0.13 × 10 ⁻³ to 5.2 × 10 ⁻³ moles of pure catalyst compound selected from the group consisting of tin, organo-titanium and organo-zirconium compounds to the reaction mixture, and (d) the catalyst compound 95% acid end, consisting of the steps of reacting the reaction mixture under atmospheric pressure at an average reaction temperature of 190 ° C.-200 ° C. for a time not exceeding 70 minutes from the time it was added to to form a directly esterified diacid product. Method for directly esterifying the above. The process of claim 1 wherein the catalyst compound of step (c) is added during step (a) to form a reaction mixture. The process of claim 2 wherein the pure catalytic compound of step (c) is added during step (a) to form a reaction mixture. The method of claim 1 or 2, wherein the diacid is selected from the group consisting of aromatic diacids and aliphatic diacids. The method of claim 1 or 2, wherein the diacid is terephthalic acid or adipic acid. The method of claim 1 or 2, wherein the diacid is terephthalic acid. The process of claim 1 wherein the catalyst compound is tetrabutyl titanate or n-butyltartrate. The process of claim 2 wherein the pure catalyst compound is tetrabutyl titanate or n-butyltin machining. The method of claim 1, wherein the ratio of 1,4-butanediol: diacid is in the range of 4: 1-6: 1. The process of claim 2 wherein the ratio of ethylene glycol: diacid is in the range of 4: 1-6: 1. The method of claim 1, wherein the average reaction temperature is in the range of 220 ° C.-230 ° C. 7. The process of claim 1 wherein the amount of catalyst compound added is from 0.36 × 10 ⁻³ to 1.7 × 10 ⁻³ mole of catalyst compound per mole of diacid. The process of claim 2 wherein the amount of pure catalyst compound added is 0.36 × 10 ⁻³ to 1.7 × 10 ⁻³ mole of catalyst compound per mole of diacid. The method of claim 1 wherein the reaction mixture is reacted for a time of no more than 30 minutes. The process of claim 1 wherein the reaction mixture is reacted under pressure at a temperature not exceeding 270 ° C. 3. The process of claim 2 wherein the reaction mixture is reacted under pressure. The process of claim 1 or 2, wherein the direct esterified diacid product comprises polycondensation into a high molecular weight polymer. The method of claim 1 or 2, further comprising the step of reacting the direct esterified diacid product to form a copolyetherester. Direct esterification of diacids with glycols in the presence of a catalyst compound selected from the group consisting of organotin, organotitanium and organozirconium compounds, consisting of the following steps (a)-(e) Semi-continuous method for polycondensation of the reaction product. (a) in a batch reactor, diacids, glycols and catalysts are mixed together and heated to a reaction temperature of at least 180 ° C. to prepare a reaction mixture, or alternatively, diacids and glycols are mixed together and reactions near 180 ° C. Heating to a temperature and adding a catalyst compound thereto to prepare a reaction mixture, (b) reacting at an average reaction temperature in the range of 180 ° C. to 245 ° C. under atmospheric pressure until at least 95% of the acid ends of the diacids are directly esterified; Reacting the mixture, (c) passing the reacted reaction mixture through a heat exchanger at a temperature of about 100 ° C.-150 ° C. to cool the mixture, (d) providing a storage capacity and continuing the reaction mixture. Passing the cooled reaction mixture to a device allowing flow, (e) the reaction mixture from the storage device is heated to at least 250 ° C. under vacuum, and polycondensed into a high molecular weight polymer Passing a heating mechanism which is passed to a separation mechanism for the polycondensation. ※ Note: The disclosure is based on the initial application.